Preparation method of zirconium oxide fibers

Abstract

The invention relates to a preparation method of zirconium oxide fibers. The preparation method comprises the following steps: preparing a precursor zirconium sol spinning solution from basic zirconium carbonate, zirconium oxychloride, glacial acetic acid, yttrium nitrate and deionized water, carrying out centrifugal spinning or electrostatic blowing to obtain zirconium oxide gel fibers, and carrying out high-temperature heat treatment to obtain zirconium oxide fibers with the diameter of 1-6[mu]m. Acording to the method, zirconium oxychloride and basic zirconium carbonate which are low in price on the market are adopted as raw materials, hydrolysis of zirconium oxychloride and the adding amount of glacial acetic acid are controlled through basic zirconium carbonate, the PH value of sol is accurately adjusted, excessive use of glacial acetic acid is avoided, zirconium oxide fibers are obtained through adoption of a centrifugal thread throwing method or an electrostatic blowing method, the preparation process is easy to operate, operation is easy, the cost is low, and large-scale production is easy.

Description

technical field [0001] The invention belongs to the technical field of inorganic refractory and energy-saving materials, and in particular relates to a preparation method of zirconia fibers. Background technique [0002] Due to its many excellent properties, polycrystalline zirconia fiber has become an important basic raw material in the fields of aerospace military industry, energy saving and emission reduction, and composite materials. Compared with other inorganic fibers, polycrystalline zirconia fibers have many unique and irreplaceable excellent properties. Among all commercially available inorganic fibers, zirconia fibers have the highest theoretical use temperature (melting point 2715°C), low thermal conductivity (the thermal conductivity of zirconia is the lowest among metal oxides), good ablation resistance, and chemical resistance. Corrosion, low vapor pressure at high temperature and high strength, it is a high-quality high-temperature heat insulation material an...

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Problems solved by technology

[0005] In-depth research has been carried out on zirconia fiber preparation technology in several domestic universities and research institutions such as Sinosteel Luoyang Refractory Research Institute Co., Ltd., Shandong University, Xiamen University, Shandong Deap Energy-saving Materials Co., Ltd., and Nanjing University of Science and Technology. Some of them have started to produce small batches of zirconia fibers; however, there are still complex production processes, poor colloidal stability, thicker diameters of prepared zirconia fibers, and serious pulverization.

[0006] In patents CN 1459418A and CN 1584155 A, zirconium oxide fibers are prepared by using zirconium oxychloride, acetylacetonate and triethylamine to synthesize zirconium acetylacetonate precursor colloid. The process is complicated and requires controlled synthesis at low temperature, which is difficult to carry out industrial production; In patents CN 102181962 B and CN 110592723 A, basic zirconium carbonate and glacial acetic acid are used, and spinning aids are added to directly synthesize precursor colloids to prepare zirconia fibers. The stability of the synthetic colloids requires excess acetic acid (1:2-3) to carry out Stable, although the patent CN110592723 A states that glacial acetic acid is used in a small amount, but the amount used still exceeds the theoretical molar reaction value (1:1) of basic zirconium carbonate and glacial acetic acid to reach 1:1.5-1.8; due to the volatility of glacial acetic acid itself , causing subsequent colloid reserves and fiber formation, acid damage to equipment and personnel